CN106986779A - A kind of preparation method of the propyl alcohol of 2 amino, 2 methyl 1 - Google Patents

A kind of preparation method of the propyl alcohol of 2 amino, 2 methyl 1 Download PDF

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CN106986779A
CN106986779A CN201710212093.8A CN201710212093A CN106986779A CN 106986779 A CN106986779 A CN 106986779A CN 201710212093 A CN201710212093 A CN 201710212093A CN 106986779 A CN106986779 A CN 106986779A
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ammonolysis
reaction
methyl
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agent
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CN106986779B (en
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奚强
马银
冯薇伟
吴忆雯
刘裴
卢洪宇
舒畅
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Wuhan Institute of Technology
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
    • C07C213/02—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/132—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group
    • C07C29/136—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH
    • C07C29/14—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of a —CHO group
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
    • C07C45/63—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by introduction of halogen; by substitution of halogen atoms by other halogen atoms

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  • Organic Chemistry (AREA)
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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention relates to a kind of preparation method of the propyl alcohol of 2 amino, 2 methyl 1, its step is as follows：1) isobutylaldehyde is dissolved in solvent and obtains isobutylaldehyde solution, at 50 DEG C, halogen source is added portionwise in isobutylaldehyde solution and reacted, question response terminates air-distillation and obtains 2 halogenated aldehydes；2) 2 halogenated aldehydes are dissolved in isopropanol, add catalyst and co-catalyst, be warming up to 60 65 DEG C of reactions, then by reaction solution rectification process, then post processing obtains 2 halohydrins；3) 2 halohydrins are subjected to ammonolysis reaction in the agent of excess of ammonia solution and ammonolysis co-catalyst, reaction solution is sloughed after ammonolysis agent, vacuum distillation, collect 102 104 DEG C of cuts (8.50 8.66KPa), obtain the propyl alcohol of 2 amino, 2 methyl 1.This method is raw materials used cheap and easy to get, and reaction condition is gentle, safe preparation process, high income, is adapted to industrialized production.

Description

A kind of preparation method of 2-amino-2-methyl-1-propanol
Technical field
The invention belongs to technical field of organic synthesis, it is related to a kind of preparation method of 2-amino-2-methyl-1-propanol.
Background technology
2-amino-2-methyl-1-propanol, abbreviation AMP is white crystals block or colourless liquid.AMP has extensive use On the way, it can be used for gas chromatographic analysis with carboxylic acid compound formation derivative, while can also improve the scrub resistance of coating, screening Gai Li, stability of viscidity and color developing etc., and can improve and strengthen many coating compositions, strengthen the effect of other auxiliary agents, In addition, AMP can be used as Biostatic and pH stable agent in metal processing sectors, AMP also has the precipitation of anti-cobalt, low bubble etc. excellent Point.
The Industrialized processing technique of existing 2-amino-2-methyl-1-propanol mainly uses 2- nitropropanes and formaldehyde Reactant aqueous solution, then concentration is the aqueous solution of -2- nitro -1- propyl alcohol of methyl containing 70%2-, and nitro compounds weight 5% is added afterwards Skeleton nickel, catalytic reaction generation 2-amino-2-methyl-1-propanol.Route raw material 2- nitropropanes are inflammable and explosive, are difficult storage Transport, and product postprocessing is complicated, purity is low.Therefore, a kind of route of new synthesis 2-amino-2-methyl-1-propanol is studied Have important practical significance.
The content of the invention
The technical problems to be solved by the invention are that there is provided a kind of 2- ammonia for above shortcomings in the prior art The preparation method of base -2- methyl isophthalic acids-propyl alcohol, this method is raw materials used cheap and easy to get, and reaction condition is gentle, safe preparation process, High income.
In order to solve the above technical problems, the technical scheme that the present invention is provided is：
A kind of preparation method of 2-amino-2-methyl-1-propanol is provided, its step is as follows：
1) 2- halogenated aldehydes are prepared：At -5-0 DEG C, halogen source is added in isobutylaldehyde and reacted, GC tracing detection isobutylaldehydes contain Amount, terminates after question response is complete, in N2Under protection, the isolated 2- halogenated aldehydes of air-distillation；
2) 2- halohydrins are prepared：By step 1) gained 2- halogenated aldehydes be dissolved in isopropanol, the 2- halogenated aldehydes and isopropanol Mol ratio is 1：3-10, adds catalyst aluminium isopropoxide and co-catalyst, is warming up to 60-65 DEG C of reaction, (DNP shows for TLC tracking For aldehyde radical and the developer of ketone group in color, thin-layer chromatography) it is complete to 2- halos aldehyde reaction, then by reaction solution rectification process, Distillation water washing is added after the acetone for removing isopropanol and reaction generation, then filtering, filtrate stratification is collected and with anhydrous Na2SO4Organic layer is dried, filtering obtains 2- halohydrins；
3) 2-amino-2-methyl-1-propanol is prepared：By step 2) gained 2- halohydrins helped in the agent of excess of ammonia solution and ammonolysis Ammonolysis reaction is carried out in catalyst, wherein ammonolysis co-catalyst consumption is the 1-10% of 2- halohydrin quality, and reaction solution sloughs ammonia Solve after agent, vacuum distillation, collect 102-104 DEG C of cut (8.50-8.66KPa), obtain 2-amino-2-methyl-1-propanol.
Preferably, the ratio between amount of material of isobutylaldehyde and halogen source is 1:1-1.5.
By such scheme, step 1) halogen source be chlorine, bromine, NCS (N- chlorosuccinimides), NBS (N- bromos Succimide) in one or more；When halogen source is NCS or NBS, isobutylaldehyde dissolving is first obtained into isobutylaldehyde with solvent molten Liquid reacts with halogen source again, and described solvent is in ether, DCM (dichloromethane), DCE (dichloroethanes), THF (tetrahydrofuran) It is one or more of.
Preferably, the isobutylaldehyde solution concentration is 2-5mol/L.
By such scheme, step 2) the 2- halogenated aldehydes and isopropanol mol ratio be 1：3-5.
By such scheme, step 2) co-catalyst be trichloroacetic acid, trifluoroacetic acid in one or more.
By such scheme, step 2) mol ratio of the 2- halogenated aldehydes, catalyst and co-catalyst is 100：5-20：0.5- 6。
Preferably, step 2) the 2- halogenated aldehydes, catalyst and co-catalyst mol ratio be 100：8-12：0.8-2.
Preferably, step 3) the ammonolysis agent mole is 3-5 times of 2- halohydrin moles.
By such scheme, step 3) the ammonolysis agent be liquefied ammonia, concentrated ammonia liquor, ammonia methanol, cholamine in one or more, When the ammonolysis agent is liquefied ammonia, the ammonolysis reaction condition is in 150-160 DEG C of reaction 5-10h under 2-4MPa pressure；It is described Ammonolysis agent be concentrated ammonia liquor when, ammonolysis reaction condition be normal pressure under in 150-160 DEG C react 20-25h；The ammonolysis agent is ammonia methanol Or during cholamine, ammonolysis reaction condition is in 130-140 DEG C of reaction 10-12h under 2-4MPa pressure.
By such scheme, step 3) the ammonolysis co-catalyst be NH4Cl、NH4Br、NH4One kind or several in I, KBr, KI Kind.
Preferably, the ammonolysis co-catalyst consumption is the 1-3% of 2- halohydrin quality.
The beneficial effects of the present invention are：What the present invention was provided prepares former used in the method for 2-amino-2-methyl-1-propanol Material is cheap and easy to get, and reaction condition is gentle, safe preparation process, high income, is adapted to industrialized production.
Embodiment
To make those skilled in the art more fully understand technical scheme, the present invention is made with reference to embodiment It is described in further detail.
Embodiment 1
A kind of preparation method of 2-amino-2-methyl-1-propanol, step is as follows：
72.1g (1mol) isobutylaldehyde is taken to be placed in the four-hole boiling flask that 250mL is equipped with thermometer, chlorination tube and device for absorbing tail gas Among, four-hole boiling flask is placed at lucifuge and is cooled to 0 DEG C；Under magnetic agitation, chlorine is passed through with 0.5L/min flow velocity, wherein logical The chlorine mouth of pipe is placed on liquid level, close at liquid level, and chlorine, which is passed through temperature at initial stage and risen to after 5 DEG C, to cool, and suitably adjusts flow velocity, control is anti- Should be interior warm at -5-0 DEG C, GC tracing detections to isobutyl aldehyde reaction completely, are reacted after terminating, in N2Under protection, air-distillation is collected 86-90 DEG C of cut, obtains intermediate 2- chloro-2-methyl -1- propionic aldehyde 96.2g, and yield is that 90.3%, GC detections product purity is 94%.
In 500mL three-necked flask, input 180.3g (3mol) isopropanol, stirring adds 106.5g (1mol) 2- Chloro-2-methyl -1- propionic aldehyde, after stirring, is weighed into 12.2g (0.06mol) aluminium isopropoxide, is sufficiently stirred for and is warming up to 60 DEG C of guarantors Temperature reaction, TLC tracing detections (DNP colour developings) are complete to the reaction of 2- chloro-2-methyl -1- propionic aldehyde, after reaction terminates, reaction solution rectifying Processing, removes the isopropanol of excess and the acetone of generation, surplus materials is added in 100mL distilled water while hot, after agitation and filtration Stratification, uses 20mL distillation water washing organic phases, washes repeatedly and merges organic phase afterwards twice, adds appropriate Na2SO4It is stirred Night, filtering collects filtrate and obtains 2- chloro-2-methyl -1- propyl alcohol 95.8g, yield is that 88.7%, GC detects that its purity is 95%.
Among 250mL three-necked flasks, 54.3g (0.5mol) 2- chloro-2-methyl -1- propyl alcohol is put into, then measure dense into 150mL Ammoniacal liquor (ammonia weight/mass percentage composition 25%), sealing is rapidly heated to 160 DEG C of reaction 6h, is cooled to room temperature, reacting liquid filtering is removed Ammonium salt, filtrate detects that raw material is substantially completely converted by GC, filtrate decompression distillation, collects 102-104 DEG C of cut (8.50- 8.66KPa), product 2-amino-2-methyl-1-propanol 30.4g is obtained, yield is 68.3%, and purity is 93%.
Embodiment 2
A kind of preparation method of 2-amino-2-methyl-1-propanol, step is as follows：
72.1g (1mol) isobutylaldehyde is taken to be placed in the four-hole boiling flask that 250mL is equipped with thermometer, chlorination tube and device for absorbing tail gas Among, 0.7g (0.04mol) water is added, four-hole boiling flask is placed at lucifuge and is cooled to 0 DEG C；Under magnetic agitation, with 0.5L/min Flow velocity be passed through chlorine, wherein chlorination tube mouthful is placed on liquid level, close at liquid level, and chlorine, which is passed through temperature at initial stage and risen to after 5 DEG C, to drop Temperature, suitably adjusts warm at -5-0 DEG C in flow velocity, control reaction, GC tracing detections are complete to isobutyl aldehyde reaction.After reaction terminates, N2Under protection, air-distillation filtrate, the cut of 86-90 DEG C of collection obtains intermediate 2- chloro-2-methyl -1- propionic aldehyde 98.6g, receives Rate is that 92.5%, GC detection product purities are 95%.
In 500mL three-necked flask, input 180.3g (3mol) isopropanol, stirring adds 106.5g (1mol) 2- Chloro-2-methyl -1- propionic aldehyde, after stirring, is weighed into 20.2g (0.1mol) aluminium isopropoxide, after being sufficiently stirred for, is warming up to 60 DEG C of guarantors Temperature reaction, TLC tracing detections (DNP colour developings) to the chloro- 1- propionic aldehyde of 2- methyl -2- have reacted.After reaction terminates, at reaction solution rectifying Reason, removes the isopropanol of excess and the acetone of generation；Surplus materials is added in 100ml distilled water while hot, quiet after agitation and filtration Layering is put, 20ml distillation water washing organic phases are used, washes repeatedly and merges organic phase afterwards twice；Add appropriate Na2SO4It is stirred overnight, Filtering, collects filtrate and obtains 2- chloro-2-methyl -1- propyl alcohol 97.4g, yield is that 90.2%, GC detection purity is 94%.
In 250mL autoclave, 54.3g (0.5mol) 2- chloro-2-methyl -1- propyl alcohol is put into, N is led in sealing2To pressure Empty, then such cyclic permutation 3 times fill ammonia to pressure 2.0MPa, be rapidly heated to 160 DEG C of reaction 30h after 0.1MPa, it is cold But to room temperature, filtering reacting liquid is to remove the ammonium salt of generation, and filtrate is detected by GC, and feed stock conversion is close to 100%, and filtrate subtracts Pressure distillation, collects 102-104 DEG C of cut (8.50-8.66KPa), obtains product 2-amino-2-methyl-1-propanol 33.5g, yield 75.1%, the purity of 2-amino-2-methyl-1-propanol is 96%.
Embodiment 3
A kind of preparation method of 2-amino-2-methyl-1-propanol, step is as follows：
At room temperature, 240mL ether is placed in three-necked flasks of the 500mL equipped with thermometer, then stirred while adding Enter 72.1g (1mol) isobutylaldehyde, N2Under protection, 0 DEG C is cooled to, 140.2g (1.05mol) NCS is added portionwise, control is added Speed, makes the temperature in whole adition process in three-necked flask be no more than 5 DEG C, and room temperature is warmed naturally to after adding stirring 10min Reaction, completely, after reaction terminates, filtering, filter cake is washed in two times with 60mL ether for GC tracking reaction to raw material isobutyl aldehyde reaction Merging filtrate, washs filtrate with the saturated aqueous common salt of 100mL ice, then adds anhydrous Na in two times afterwards2SO4It is stirred overnight, mistake Filter, filtrate is in N2Under protection, air-distillation, the cut of 86-90 DEG C of collection obtains 2- chloro-2-methyl -1- propionic aldehyde 102.1g, yield It is 96% for 95.8%, GC detection product purities.
In 500mL three-necked flask, input 180.3g (3mol) isopropanol, stirring adds 106.5g (1mol) 2- Chloro-2-methyl -1- propionic aldehyde, after stirring, is weighed into 16.3g (0.08mol) aluminium isopropoxides and the chloroethenes of 1.31g (0.008mol) three Acid, after being sufficiently stirred for, is warming up to 60 DEG C of insulation reactions, TLC tracing detections (DNP colour developings) to the chloro- 1- propionic aldehyde reactions of 2- methyl -2- Complete, after reaction terminates, reaction solution rectification process removes the isopropanol of excess and the acetone of generation, and surplus materials is added while hot In 100mL distilled water, stratification after agitation and filtration uses 20mL distillation water washing organic phases, washes and is associated with afterwards twice repeatedly Machine phase, adds appropriate Na2SO4It is stirred overnight, filters, collects filtrate and obtain 2- chloro-2-methyl -1- propyl alcohol 99.9g, yield is 92.5%, GC detection purity are 96%.
In 250mL autoclave, 54.3g (0.5mol) 2- chloro-2-methyl -1- propyl alcohol is put into, then measure the first into 100mL N is led in alcohol, sealing2Emptied after to pressure 0.1MPa, such cyclic permutation 3 times, after fill ammonia to pressure 2.0MPa, very short Temperature is promoted to 140 DEG C in time, insulation reaction 12h, cooling, reacting liquid filtering turns except the ammonium salt of generation, filtrate GC detections Rate nearly 97%, vacuum distillation collects 102-104 DEG C of cut (8.50-8.66KPa), obtains product 2- amino-2-methyls -1- third Alcohol 35.9g, yield 80.5%, purity 99%.
Embodiment 4
A kind of preparation method of 2-amino-2-methyl-1-propanol, step is as follows：
At room temperature, 240mLDCM is added in the 500mL three-necked flask equipped with thermometer, then stir while Add 72.1g (1mol) isobutylaldehyde, N20 DEG C is cooled under protection, 186.9g (1.05mol) NBS is added portionwise, control is added Speed, makes the temperature in whole adition process in three-necked flask be no more than 5 DEG C, and room temperature is warmed naturally to after adding stirring 10min Reaction, GC tracking reaction to raw material isobutyl aldehyde reaction completely, is reacted after terminating, filtering, after filter cake is washed in two times with 60mLDCM Merging filtrate, is applied mechanically again after 50 DEG C of vacuum drying of filter cake with NaBrO reaction generations NBS；Filtrate is eaten with the saturation of 100mL ice Salt solution is washed in two times, then adds anhydrous Na2SO4It is stirred overnight, filters, filtrate is in N2Under protection, air-distillation is collected 100-105 DEG C of cut, obtains the bromo- 2- methyl isophthalic acids-propionic aldehyde 142.3g of 2-, and yield is that 94.3%, GC detection product purities are 95%.
Into 500mL three-necked flask, isopropanol 180.3g (3mol) is added, stirring adds 150.9g (1mol) 2- Bromo- 2- methyl isophthalic acids-propionic aldehyde, after stirring, is weighed into 12.2g (0.06mol) aluminium isopropoxide, is sufficiently stirred for, is warming up to after 60 DEG C Insulation reaction, TLC tracing detections (DNP colour developings) to the bromo- 2- methyl isophthalic acids of 2--propionic aldehyde reaction is complete, after reaction terminates, reaction solution essence Processing is evaporated, the isopropanol of excess and the acetone of generation is removed, surplus materials is added in 100mL distilled water while hot, agitation and filtration Stratification, uses 20mL distillation water washing organic phases afterwards, washes repeatedly and merges organic phase afterwards twice, adds appropriate Na2SO4Stirring Overnight, filter, collect filtrate and obtain the bromo- 2- methyl isophthalic acids-propyl alcohol 129.3g of 2-, yield is that 84.5%, GC detects that its purity is 96%.
In 250mL autoclave, the bromo- 2- methyl isophthalic acids-propyl alcohol of 76.5g (0.5mol) 2- is put into, then measure the first into 100mL N is led in alcohol, sealing2Emptied after to pressure 0.1MPa, such cyclic permutation 3 times, fill ammonia to internal pressure 2.0MPa, when very short Interior that temperature is promoted into 140 DEG C, insulation reaction 12h, cooling, reacting liquid filtering is converted except the ammonium salt of generation, filtrate GC detections Rate nearly 97%, filtrate decompression distillation, collects 102-104 DEG C of cut (8.50-8.66KPa), obtains product 2- amino-2-methyls -1- Propyl alcohol 36.3g, yield 81.4%, purity 99%.
Embodiment 5
A kind of preparation method of 2-amino-2-methyl-1-propanol, step is as follows：
2- chloro-2-methyl -1- propyl alcohol is prepared using method same as Example 1.
In 250mL autoclave, input 54.3g (0.5mol) 2- chloro-2-methyl -1- propyl alcohol and ammonium chloride 1.34g (0.025mol) and 0.54gKCI, then the methanol into 100mL is measured, seal, lead to N2Emptied after to pressure 0.1MPa, so circulation is put Change 3 times, after fill ammonia to pressure 2.0MPa, temperature is promoted to 140 DEG C in a short period of time, insulation reaction 12h, cooling, Reacting liquid filtering collects 102-104 DEG C of cut except the ammonium salt of generation, filtrate GC detections, conversion ratio nearly 98%, filtrate decompression distillation (8.50-8.66KPa), weigh 38.4g, yield 86.2%, purity 99%.

Claims (7)

1. a kind of preparation method of 2-amino-2-methyl-1-propanol, it is characterised in that step is as follows：
1) 2- halogenated aldehydes are prepared：At -5-0 DEG C, halogen source is added in isobutylaldehyde and reacted, the amount of the material of isobutylaldehyde and halogen source The ratio between be 1:1-1.5, GC tracing detection isobutyraldehyde content, terminate after question response is complete, in N2Under protection, air-distillation is separated To 2- halogenated aldehydes；
2) 2- halohydrins are prepared：By step 1) gained 2- halogenated aldehydes are dissolved in isopropanol, the 2- halogenated aldehydes and isopropanol mole Than for 1：3-10, adds catalyst aluminium isopropoxide and co-catalyst, is warming up to 60-65 DEG C of reaction, it is anti-that TLC tracks to 2- halogenated aldehydes Should be complete, then by reaction solution rectification process, distillation water washing, subsequent mistake are added after the acetone for removing isopropanol and reaction generation Filter, filtrate stratification is collected and uses anhydrous Na2SO4Organic layer is dried, filtering obtains 2- halohydrins；
3) 2-amino-2-methyl-1-propanol is prepared：By step 2) gained 2- halohydrins in the agent of excess of ammonia solution and ammonolysis co-catalysis Ammonolysis reaction is carried out in agent, wherein ammonolysis co-catalyst consumption is the 1-10% of 2- halohydrin quality, and reaction solution sloughs ammonolysis agent Afterwards, vacuum distillation, obtains 2-amino-2-methyl-1-propanol.
2. preparation method according to claim 1, it is characterised in that step 1) halogen source is chlorine, bromine, NCS, NBS In one or more；When halogen source be NCS or NBS when, first with solvent by isobutylaldehyde dissolving obtain isobutylaldehyde solution again with halogen source Reaction, described solvent is the one or more in ether, DCM, DCE, THF.
3. preparation method according to claim 1, it is characterised in that step 2) the 2- halogenated aldehydes and isopropanol mol ratio For 1：3-5.
4. preparation method according to claim 1, it is characterised in that step 2) co-catalyst is trichloroacetic acid, trifluoro One or more in acetic acid.
5. preparation method according to claim 1, it is characterised in that step 2) the 2- halogenated aldehydes, catalyst and co-catalysis The mol ratio of agent is 100：5-20：0.5-6.
6. preparation method according to claim 1, it is characterised in that step 3) the ammonolysis agent is liquefied ammonia, concentrated ammonia liquor, ammonia One or more in methanol, cholamine, when the ammonolysis agent is liquefied ammonia, the ammonolysis reaction condition is under 2-4MPa pressure 5-10h is reacted in 150-160 DEG C；The ammonolysis agent be concentrated ammonia liquor when, ammonolysis reaction condition be normal pressure under in 150-160 DEG C reaction 20-25h；When the ammonolysis agent is ammonia methanol or cholamine, ammonolysis reaction condition is anti-in 130-140 DEG C under 2-4MPa pressure Answer 10-12h.
7. preparation method according to claim 1, it is characterised in that step 3) the ammonolysis co-catalyst is NH4Cl、 NH4Br、NH4One or more in I, KBr, KI.
CN201710212093.8A 2017-04-01 2017-04-01 A kind of preparation method of 2-amino-2-methyl-1-propanol Expired - Fee Related CN106986779B (en)

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